Microchimica Acta

, Volume 182, Issue 15–16, pp 2521–2528 | Cite as

Removal of acidic interferences in multi-pesticides residue analysis of fruits using modified magnetic nanoparticles prior to determination via ultra-HPLC-MS/MS

  • Peipei Qi
  • Zhiwei Wang
  • Guiling Yang
  • Chunqing Shang
  • Hao Xu
  • Xiangyun Wang
  • Hu Zhang
  • Qiang Wang
  • Xinquan WangEmail author
Original Paper


The authors describe magnetite (Fe3O4) nanoparticles modified with 3-(N,N-diethylamino) propyltrimethoxysilane (Fe3O4-PSA NPs) for use as a sorbent for dispersive solid phase extraction of pesticide residues. The Fe3O4-PSA NPs were prepared by silanizing Fe3O4 NPs and modifying them with 3-(N,N-diethylamino) propyltrimethoxysilane. Field-emission scanning electron microscopy, FTIR and zeta potential measurements were employed to characterize the modified NPs. They were then used as an adsorbent to remove acidic interferences (such as malic acid and succinic acid), which are major interferences in LC-MS/MS analysis in causing ion suppression in the MS spectra of pesticides. In addition, graphitized carbon black (GCB) was used as an adsorbent to eliminate interferences by pigments. The use of Fe3O4-PSA NPs can replace time-consuming centrifugation as used in the so-called QuEChERS (quick, easy, cheap, effective, rugged and safe) method. This improvement is particularly significant in high-throughput analysis. Following the optimization of the quantities of Fe3O4-PSA NPs and GCB, the method was applied to the determination of 56 pesticides in (spiked) fruits (apple, kiwi, orange and pear) by ultra-HPLC-MS/MS. The analytical ranges typically extend from 1 to 200 ng∙mL−1, and recoveries range from 60.2 to 130 % at different concentrations of all four kinds of fruits. The LOQs for the pesticides are 10 ng∙kg−1, which makes the method a viable tool for pesticide monitoring in fruits.

Graphical Abstract

Magnetite nanoparticles modified with 3-(N,N-diethylamino) propyltrimethoxysilane (Fe3O4-PSA NPs) are shown to be useful materials for removal of acidid interferents from sample matrices. Their use can replace time-consuming centrifugation as used in the traditional QuEChERS method.


Magnetite nanoparticles Dispersive solid phase extraction Pesticides residue Organic acid Ultra high performance liquid Chromatography Mass spectrometry 



This study was supported by grants from Zhejiang Provincial Natural Science Foundation of China (Grant No. LQ15B050001), the analysis and test foundation of Zhejiang Province (Grant No. 2014C37053), the Special Fund for Agro-scientific Research in the Public Interest (Grant No. 201503107-12) and the Ministry of Science and Technology of the People’s Republic of China (Grant No. 2011AA100806).

Supplementary material

604_2015_1615_MOESM1_ESM.doc (3.5 mb)
ESM 1 (DOC 3607 kb)


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Copyright information

© Springer-Verlag Wien 2015

Authors and Affiliations

  • Peipei Qi
    • 1
    • 3
  • Zhiwei Wang
    • 1
    • 3
  • Guiling Yang
    • 1
    • 3
  • Chunqing Shang
    • 2
  • Hao Xu
    • 1
    • 4
  • Xiangyun Wang
    • 1
    • 4
  • Hu Zhang
    • 1
    • 5
  • Qiang Wang
    • 1
    • 5
  • Xinquan Wang
    • 1
    • 3
    Email author
  1. 1.Institute of Quality and Standard of Agro-productsZhejiang Academy of Agricultural SciencesHangzhouPeople’s Republic of China
  2. 2.Shanghai Enriching Biotechnology LtdShanghaiPeople’s Republic of China
  3. 3.State Key Laboratory Breeding Base for Zhejiang Sustainable Pest and Disease ControlHangzhouPeople’s Republic of China
  4. 4.Agricultural Ministry Key Laboratory for Pesticide Residue DetectionHangzhouPeople’s Republic of China
  5. 5.Key Laboratory of Detection for Pesticide Residues and Control of ZhejiangHangzhouPeople’s Republic of China

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